42results about How to "The catalytic system is simple" patented technology

The invention discloses a method for preparing a 1, 2, 3-triazole compound. The technical scheme of the invention is as follows: the method for preparing the 1, 2, 3-triazole compound comprises the following steps: (1), weighing copper acetate and Pullulan respectively, fully dissolving the copper acetate and the Pullulan in water, wherein the copper acetate is Cu(OAc)2.H2O; and (2), adding a terminal alkyne compound and an azide compound at 70-100 DEG C while stirring, keeping the temperature till the end of reaction, cooling, separating out a solid, filtering, and purifying to obtain the 1, 2, 3-triazole compound. The using amount of the copper in a catalytic system is reasonable and the defect that a ligand is high in toxicity is overcome, so that the method for preparing the 1, 2, 3-triazole compound is an environment-friendly method.

The invention discloses a convenient and efficient preparation method of benzofuran or indole. The preparation method comprises the following steps of: reacting various natural or non-natural aldehyde ketone with sulfonylhydrazine to obtain corresponding hydrazone; and reacting the hydrazone with substituted ortho-hydroxybenzene acetylene or substituted ortho-aminobenzene acetylene in a basic condition by using a copper compound as a catalyst in an organic solvent to obtain the derivative of benzofuran or indole. The method has wide substrate adaptability, can be used for synthesizing various benzofuran or indole compounds carrying different substituents, uses the copper compound with low price as a catalyst, has low price and easily available initial raw materials in the reaction, namely aldehyde ketone and ortho-hydroxybenzene acetylene or ortho-aminobenzene acetylene, as well as is convenient operation in the reaction process, and is suitable for large-scale synthesis.

The invention provides an olefin polymerization catalyst composition comprising a nitrogen-containing heterocyclic ligand compound as shown in formula I, a transition metal compound and a cocatalyst; and R1, R2, R3 and R4 can be independently selected from hydrogen, alkyl, or alkoxy. The invention also provides an application method of the catalyst composition, including olefin polymerization of olefins in the presence of the catalyst composition and an organic solvent in a reactor.

The invention discloses a preparation method of 1,2,3-triazole compound and belongs to the field of medicament catalyzed synthesis technology. The technical scheme is characterized in that according to the preparation method of the 1,2,3-triazole compound, an end group alkyne compound and organic trinitride are respectively used as raw materials; pullulan triazole / cuprous chloride is used as a catalytic system; water is used as a solvent; the 1,2,3-triazole compound is prepared through mixed stirring reaction under the condition of the room temperature of minus 100 DEG C. According to the preparation method, pullulan polymer cotaining triazole group is applied to Huisgen cycloaddition reaction to be used as an additive to stabilize cuprous ions so that use level of catalyst in the catalytic reaction process is reduced. The catalytic system is mainly subjected to catalytic reaction in water, simple, reliable, high in yield, easy to separate, reusable, green, environmentally friendly, and the like.

The invention discloses a method for preparing aldehyde or ketone by copper salt / bidentate ligand / TEMPO catalytic air oxidation alcohol. The alcohol is used as a raw material, an organic solution is used as a solvent, and the air is used as an oxidant. The raw material alcohol is oxidized to obtain the corresponding aldehyde or ketone under the catalysis of the copper salt / bidentate ligand / TEMPO. The copper salt / bidentate ligand / TEMPO catalytic air oxidation alcohol is utilized. A technical route has the advantages of simplifying a catalytic system, being simple in operation, good in substrate applicability, high in yield, low in cost and easy to industrialize, so that the method is a very economical simple method for preparing the aldehyde or the ketone from the alcohol.

The invention relates to a synthetic method of an asymmetric disulfide compound. According to the method, mercaptan which is convenient and easy to obtain and symmetrical disulfide compounds are usedas raw materials, and the asymmetric disulfide compounds are efficiently synthesized under the catalytic action of palladium salt or copper salt. The method has the advantages of accessible raw materials, simple catalytic system, high functional group compatibility, high yield and the like, and is convenient to operate. The method is particularly suitable for selectively introducing disulfide bonds into complex substrates, and can be widely applied to the industries of medicines, foods and the like.

The invention relates to a synthetic method of aryl-alkyl thioether. According to the synthetic method, with aryl metal organic sulfinate (ArSO2M or (ArSO2)2M) as an arylation reagent and alkyl sulfhydryl as a reaction substrate, aryl-alkyl thioether is obtained under the actions of catalyzer and alkali. The aryl metal organic sulfinate is sodium salt, kali salt, lithium salt, silver salt, zinc salt and copper salt of aryl sulfinate. The aryl metal organic sulfinate is a arylation reagent with high efficiency and good universality.

An organic catalyst system for selectively oxidizing hydrocarbon to obtain oxygen- contained compound (ketone, alcohol, or acid) is proportionally prepared from o-phenanthroline compound, Br moleculae and N-hydroxy phthalic imidine. It has low toxin and low pollution.

The invention discloses indole[3,2-c]quinoline compounds represented by formula I or pharmaceutically acceptable salts thereof, and a preparation method and an application thereof, and belongs to the technical field of the pharmaceutical chemistry. The indole[3,2-c]quinoline compounds or pharmaceutically acceptable salts thereof have a very good tubercle bacillus resisting activity, and the MIC value of the most compounds is 2.5mug / mL.

The invention discloses a photocatalytic synthesis method of a C2 substituted 2H-benzothiazole hydroxyl alkylation derivative. The method comprises the following steps of: mixing substituted 2H-benzothiazole shown as a formula (II) with fatty alcohol shown as a formula (III), adding an oxidizing agent Selectfluor, an additive trifluoroacetic acid and a solvent acetonitrile, and carrying out a normal temperature stirring reaction under the protection of nitrogen and the irradiation of an LED blue light lamp; carrying out TLC monitoring until the reaction is finished, and carrying out separationand purification on the reaction liquid to obtain the C2-substituted 2H-benzothiazole hydroxyalkylated derivative represented by formula (I). The invention provides a new method for synthesizing the2H-benzothiazole C2 hydroxyalkylated derivative through visible light induction by taking Selectfluor as an oxidizing agent, trifluoroacetic acid as an additive and acetonitrile as a solvent. The method is simple in catalytic system, mild in reaction condition and wide in substrate range.

The invention discloses a preparation method of a C2 substituted 2Hbenzothiazole acylation derivative. The preparation method comprises the following steps: mixing 2Hbenzothiazole with substituted methyl benzene, adding an oxidizing agent K2S2O8, reacting in an air atmosphere, carrying out TLC (Thin Layer Chromatography) monitoring until the reaction is finished, and separating and purifying the reaction solution to obtain the C2 substituted 2Hbenzothiazole acylation derivative. By the adoption of the technology, K2S2O8 serves as an oxidizing agent, the C2-substituted 2Hbenzothiazole acylationderivative is synthesized through a heating reaction in the air atmosphere, and the method is simple in catalytic system, good in product yield, wide in substrate range and suitable for application and popularization.

The invention discloses a method for jointly producing biodiesel and lactic acid, comprising the following steps: mixing grease with short-chain alcohol; preheating the mixture until the temperature of the mixture is 60-90 DEG C; adding the heated mixture into a reactor; utilizing solid base to catalyze an ester exchange reaction, and carrying out phase splitting to obtain coarse biodiesel, byproduct glycerol and solid base catalyst; mixing the byproduct glycerol with water to form a glycerol aqueous solution; adding the roasted sodium silicate, evenly mixing, then causing the mixture to react at the temperature of 200-350 DEG C for 30-120min; causing the reaction product lactate to be replaced to obtain the lactic acid, wherein waste acid liquor is utilized as a compound fertilizer raw material or a building raw material; and the recycled short-chain alcohol and the roasted sodium silicate can be used repeatedly. The method disclosed by the invention has the advantages that reutilization of activity-dip catalyst and the high value-added development of the byproduct glycerol can be realized; an economically feasible process for jointly producing the biodiesel and the lactic acid can be provided; and the preparation process is simple, the byproduct glycerol is converted into the lactic acid, the production cost for the biodiesel can be obviously lowered, and the market competitive power of the biodiesel is enhanced.

The invention discloses a C2 substituted 2H-benzothiazole aryl acylated derivative, and a synthesis method and application thereof. The preparation method of the derivative comprises the following steps: mixing substituted 2H-benzothiazole and substituted methyl benzene, adding into a solvent, in the presence of an oxidizing agent Selectfluor and an additive trifluoroacetic acid, carrying out a heating and stirring reaction in the air atmosphere, performing TLC monitoring is conducted till the reaction is finished, and separating and purifying the obtained reaction liquid to obtain the target product C2 substituted 2H-benzothiazole aryl acylated derivative. The substituted methyl benzene used in the invention is low in price, easy to obtain and good in chemical stability, the method has the advantages of being high in atom economy, simple in catalytic system, free of transition metal catalysts, good in product yield, wide in substrate range and the like, and the prepared compound structure can be further optimized as an anti-tumor drug lead.

The invention discloses a mild photocatalytic synthesis method of a C2 ether substituted 2H-benzothiazole derivative. The preparation method comprises the following steps: mixing 2H-benzothiazole shown as a formula (II) with ether shown as a formula (III); adding an oxidizing agent Selectfluor, an additive trifluoroacetic acid and a solvent acetonitrile, carrying out a normal temperature stirringreaction under the protection of nitrogen and the irradiation of an LED blue light lamp, carrying out TLC monitoring until the reaction is finished, and carrying out separation and purification on thereaction liquid to obtain the C2 ether substituted 2H-benzothiazole derivative represented by the formula (I). The invention provides a new method for synthesizing the C2 ether substituted 2H-benzothiazole derivative through visible light induction by taking Selectfluor as an oxidizing agent, trifluoroacetic acid as an additive and acetonitrile as a solvent, and the method has the advantages of simple catalytic system, mild reaction conditions, wide substrate range and the like.

The invention discloses a method for preparing biodiesel under catalysis of ionic liquid. The method comprises the following steps of: mixing the ionic liquid, short-chain alcohol and free fatty acid or high-acid-value oil and fat to perform a reaction at a certain temperature; and synthesizing fatty acid methyl ester, namely the biodiesel or synthesizing the biodiesel by a two-step method. The conventional ionic liquid is low in cost and the activity of the ionic liquid is obviously improved within the limited reaction temperature range, so the ionic liquid can be separated, recovered and reused easily after the reaction is finished. The method has the characteristics of simple catalytic system, reusability and simple process.

The invention discloses a preparation method of an amino-acid ester or deuterated amino-acid ester compound, which comprises the following steps of: adding a photosensitizer and an organic solvent into a reaction container by taking imidic ester, silane and water or heavy water as initial raw materials, carrying out stirring reaction under the irradiation of blue light, detecting that the reaction raw material imidic ester completely disappears by TLC thin-layer chromatography, and filtering to obtain the deuterated amino-acid ester compound. And stopping stirring, removing the volatile solvent, carrying out silica gel column chromatography or neutral alumina column chromatography, and carrying out vacuum concentration to obtain the target amino-acid ester or deuterated amino-acid ester compound. According to the method, blue light catalysis is used for replacing traditional precious metal catalysis, silane and water are used for replacing a traditional hydrogen source for the first time, transfer hydrogenation of the imidic ester compounds is achieved, cheap deuterium water is used as a deuterium source, a series of deuterated amino-acid ester compounds can be prepared, and therefore the production cost is greatly reduced; the method provided by the invention has the advantages of mild catalytic conditions, simple catalytic system, high reaction selectivity, high safety and high synthesis efficiency, and is worthy of popularization and application.

The invention discloses a preparation method of a nitro-substituted indole compound. The method comprises the following steps: mixing a dinitrobenzene compound and an enaminone compound according to amolar ratio of (1-3): (1-3); carrying out a stirring reaction on the mixture in an air atmosphere at a temperature of 25-150 DEG C in the presence of m-dichlorobenzene (MCB) as a solvent and an alkali promoter for 12-24 h; carrying out TLC detection to determine the reaction process, and after the reaction is finished, washing the reaction solution with water, extracting, drying and carrying outcolumn chromatography separation to obtain a target product. The method provided by the invention has the advantages of cheap and easily available raw materials, simple and mild catalytic conditions,convenient post-treatment, a high yield and the like, and the obtained product has good economic added value and certain economic benefits.

The invention discloses a preparation method of a C2-substituted 2H-benzothiazole hydroxyalkylated derivative. The preparation method comprises the following steps: mixing substituted 2H-benzothiazolewith fatty alcohol, taking an organic dye photosensitizer as a catalyst, carrying out a normal-temperature stirring reaction in a solvent under the protection of nitrogen and the irradiation of an LED white light lamp, carrying out TLC monitoring until the reaction is finished, and carrying out separation and purification on a reaction solution to obtain the C2-substituted 2H-benzothiazole hydroxyalkylated derivative. By adopting the technology, a cheap and readily available organic dye is used as the catalyst, the new method for synthesizing the 2H-benzothiazole C2 hydroxyalkylated derivative through visible light induction is simple in catalytic system, mild in reaction condition, cheap and readily available in catalyst and good in yield.

The invention provides a method for preparing lactic acid by hydrolyzing biomass, and the method realizes the purpose of preparing the lactic acid through hydrolization under the action of an acidic catalyst by taking biomass as a raw material, water as a reaction solvent and a salt of trifluoromethanesulfonic acid as a catalyst. The method provided by the invention has the advantages of simple preparation process, easiness for raw material obtaining, quick reaction, high catalyst activity, few byproduct, resource conservation and cost reduction because the catalyst can be recycled through extraction, important application value and suitability for industrialized production and application; and according to the invention, the process is environmentally-friendly without pollution, a catalyzing system is relatively simple, the raw material conversion rate can achieve 100%, and the lactic acid yield can maximally achieve 98.2%.

The invention belongs to the technical field of pharmaceutical chemistry, and discloses a Toddacoumalone compound or a pharmaceutically acceptable salt and a preparation method and application thereof. The general formula of the molecular structure of the Toddacoumalone compound is shown in the formula I or the formula II or formula II. The provided Toddacoumalone compound has good anti-phosphodiesterase 4 activity. According to the preparation method of the Toddacoumalone compound, a simple and easy-to-obtain quinolinone substrate and an aldehyde compound are used as raw materials, the reaction step is short, and the yield is relatively high. The preparation method has the advantages that the reaction substrate is easy to obtain, a catalytic system is simple, operation is simple, the functional group tolerance is good, the compound is economical and effective and the product structure is diversified and has very important academic value and further application and popularization significance.

The invention discloses a preparation method of cyclic carbonate and a preparation method of a catalyst, and belongs to the technical field of green catalytic synthesis. The invention designs an artificially synthesized organic catalyst derived from a natural alpha-amino acid raw material. R2 groups in the catalyst are side chain R groups of glycine, valine, phenylglycine and phenylalanine, a catalyst structure with better activity is obtained through a preliminary screening experiment, R1 and R3 groups in the catalyst structure are further modified, and the catalyst with optimal activity is screened out. Finally, through reaction condition optimization and substrate range screening, the efficient catalytic activity of the organic catalyst for catalyzing epoxide to prepare cyclic carbonate under mild conditions is verified.

The invention discloses a preparation method of N-formamide compounds. Carbon dioxide and organic amines are used as raw materials, hydrogen-containing silane is added as a reducing agent, and a 0.1-1.0 mol% salen-type metal complex is used as a catalyst. Under the conditions of 0.1-5.0 MPa and a temperature of 25-100 ° C, with or without adding a co-catalyst, synthesize N-formamide organic compounds; after the reaction, add an organic solvent, centrifuge, separate the catalyst, and pass the supernatant through After the solvent is removed by rotary evaporation, N-formamide compounds are obtained. The preparation method has the advantages of mild reaction conditions, no need to add any organic solvent, simple operation, high catalytic activity, good substrate compatibility, etc., conforms to a green synthesis process, and is suitable for industrial production. In addition, the catalytic system provided by the present invention can be conveniently separated from the reaction system by adding a solvent, so as to realize the recycling of the catalyst.

The invention discloses a C2 substitution 2 H -Preparation method of benzothiazole acylated derivatives. The preparation method is as follows: 2 H - Benzothiazole is mixed with the substituted methylbenzene of the oxidant K 2 S 2 O 8 , carry out the reaction in the air atmosphere, after TLC monitoring to the end of the reaction, the reaction solution is separated and purified to obtain C2 substituted 2 H - Benzothiazole Acylated Derivatives. The present invention uses the above-mentioned technology to achieve K 2 S 2 O 8 Synthetic C2-substituted 2 for oxidizing agent, heated and reacted in air atmosphere H A new method for acylation of benzothiazole derivatives, the method has simple catalytic system, good product yield and wide substrate range, and is suitable for popularization and application.

The invention discloses a method for preparing a 1, 2, 3-triazole compound. The technical scheme of the invention is as follows: the method for preparing the 1, 2, 3-triazole compound comprises the following steps: (1), weighing copper acetate and Pullulan respectively, fully dissolving the copper acetate and the Pullulan in water, wherein the copper acetate is Cu(OAc)2.H2O; and (2), adding a terminal alkyne compound and an azide compound at 70-100 DEG C while stirring, keeping the temperature till the end of reaction, cooling, separating out a solid, filtering, and purifying to obtain the 1, 2, 3-triazole compound. The using amount of the copper in a catalytic system is reasonable and the defect that a ligand is high in toxicity is overcome, so that the method for preparing the 1, 2, 3-triazole compound is an environment-friendly method.

The invention belongs to the technical field of acid anhydride preparation, and particularly relates to a method for preparing acid anhydride through catalytic dehydration of a carboxylic acid compound. According to the preparation method, under the condition that an N-N bidentate ligand is adopted as a catalyst, a carboxylic acid compound is heated in an inert solvent, intramolecular dehydration condensation of the carboxylic acid compound is catalyzed, and the target anhydride compound is obtained at a high yield. The method has the advantages that the catalytic system is simple, the catalytic effect is good when the catalyst amount is small, and the substrate adaptability is good; the reaction speed and the conversion rate are high; the method has the advantages of simple reaction operation and post-treatment steps, mild conditions, solvent recovery and repeated use, no pollution in the reaction process and the like, can be widely used for production and application, and has great significance in the synthesis field of carboxylic acid anhydride.

The invention discloses a photocatalytic synthesis method of C2-substituted 2H-benzothiazole hydroxyl alkylated derivatives. It comprises the steps of: mixing substituted 2H-benzothiazole shown in formula (II) with aliphatic alcohol shown in formula (III), adding oxidant Selectfluor, additive trifluoroacetic acid, solvent acetonitrile, under nitrogen protection and LED Carry out stirring reaction at normal temperature under the irradiation of blue light, after TLC monitors to the end of reaction, the reaction solution is separated and purified to obtain C2 substituted 2H-benzothiazole hydroxyalkylated derivatives as shown in formula (I); the invention provides a A new method for the synthesis of 2H-benzothiazole C2 hydroxyalkylated derivatives induced by visible light using Selectfluor as an oxidant, trifluoroacetic acid as an additive, and acetonitrile as a solvent. The method has a simple catalytic system, mild reaction conditions, and a wide range of substrates wide.

The invention belongs to the technical field of organic synthetic chemistry. According to the method, ethyl diazoacetate and arylboronic acid are used as coupling reagents and a 1,1-arylation alkylation reaction is carried out with catalysis of copper, thereby synthesizing the important (E)-beta-aryl-beta,gamma-unsaturated ester in one step. The method specifically comprises the following steps:mixing an alkyne compound, a solvent, ethyl diazoacetate, an arylboronic acid compound, phenanthroline, CuI and K3PO4, then carrying out closed reaction for 1.2-3 hours at 90-110 DEG C in an inert gasatmosphere; and after the reaction is finished, carrying out post-treatment to obtain the product. The method has the characteristics of simple catalytic system, cheap and easily available raw materials, excellent functional group compatibility, high region and chemical selectivity, wide substrate application range and the like, and is suitable for synthesizing various (E)-beta-aryl-beta,gamma-unsaturated ester compounds.